JPH076967B2 - Molecular weight distribution analysis method for polyketone - Google Patents
Molecular weight distribution analysis method for polyketoneInfo
- Publication number
- JPH076967B2 JPH076967B2 JP20060390A JP20060390A JPH076967B2 JP H076967 B2 JPH076967 B2 JP H076967B2 JP 20060390 A JP20060390 A JP 20060390A JP 20060390 A JP20060390 A JP 20060390A JP H076967 B2 JPH076967 B2 JP H076967B2
- Authority
- JP
- Japan
- Prior art keywords
- polyketone
- molecular weight
- weight distribution
- dichloroacetic acid
- analysis method
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Lifetime
Links
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- Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
Description
【発明の詳細な説明】 〔産業上の利用分野〕 本発明はポリケトンの分子量分布分析法に関する。さら
に詳しくは，ゲルバーミエーションクロマトグラフィを
用いたポリケトンの品質管理・性能評価等の好適な分子
量分析法に関する。TECHNICAL FIELD The present invention relates to a molecular weight distribution analysis method for polyketones. More specifically, it relates to a suitable molecular weight analysis method such as quality control and performance evaluation of polyketone using gel permeation chromatography.
ポリケトンの特徴として，下記の点が挙げられる。１）
抜群の耐薬品性。２）熱変形温度が非常に高い（326
℃）。３）高強度及び高剛性。４）低発煙，低毒性。The characteristics of polyketone are as follows. 1)
Outstanding chemical resistance. 2) The heat distortion temperature is very high (326
C). 3) High strength and high rigidity. 4) Low smoke and low toxicity.
これらの特徴を生かして，ポリケトンは化学プラント，
航空宇宙，ベアリング，ワイヤ，ケーブルなどに使用さ
れている。Taking advantage of these characteristics, polyketones are used in chemical plants,
Used in aerospace, bearings, wires, cables, etc.
これらの各用途に要求されるポリケトンの品質も様々で
あり，これに応じてポリケトンの品質を管理する必要が
ある。The quality of the polyketone required for each of these applications is also various, and it is necessary to control the quality of the polyketone accordingly.
しかしながら，ポリケトンは上記のように耐薬品性に優
れており，今までポリケトンを溶解する適当な溶媒がな
く，ポリケトンの分子量分布測定は行われていなかっ
た。However, polyketone is excellent in chemical resistance as described above, and there has been no suitable solvent for dissolving polyketone until now, and the molecular weight distribution of polyketone has not been measured.
上記の課題を解決するため，この発明はポリケトンの品
質管理や性能評価が可能な分析法を提供しようとするも
のである。In order to solve the above-mentioned problems, the present invention aims to provide an analytical method capable of quality control and performance evaluation of polyketone.
本件発明者は，鋭意検討の結果，ポリケトンはジクロロ
酢酸に加熱溶解することを見いだし発明をなすに至っ
た。As a result of intensive studies, the present inventor has found that polyketone is heated and dissolved in dichloroacetic acid, and has completed the invention.
すなわち，本発明はポリケトンの溶解液としてジクロロ
酢酸を用い，ゲルパーミエーションクロマトグラフィ
（以下GPCという）の移動相としてジクロロ酢酸を用
い，検出手段として示差屈折計を用いて分析することを
特徴とする。That is, the present invention is characterized in that dichloroacetic acid is used as a solution of a polyketone, dichloroacetic acid is used as a mobile phase of gel permeation chromatography (hereinafter referred to as GPC), and a differential refractometer is used as a detection means.
GPCは，例えば多孔性スチレン−ジビニルベンゼン系重
合体球状微粒子を充てん剤としたカラムに，分析しよう
とする試料を移動相溶媒に溶解させた溶液を付し，試料
分子の大きいものから順に分子のサイズ別に分離させ，
試料分子を分析するものである。GPC is, for example, a column containing porous styrene-divinylbenzene polymer spherical particles as a packing material, and a solution prepared by dissolving the sample to be analyzed in a mobile phase solvent. Separate by size,
It analyzes sample molecules.
本発明において，ポリケトンがジクロロ酢酸に加熱溶解
されて注入用溶液が調整された後，これがジクロロ酢酸
を移動相とするGPCに付される。この場合，ポリケトン
溶解用ジクロロ酢酸と移動相のジクロロ酢酸とは同一で
あることが，装置の操作上好ましい。In the present invention, a polyketone is heated and dissolved in dichloroacetic acid to prepare an injection solution, which is then subjected to GPC using dichloroacetic acid as a mobile phase. In this case, it is preferable for the operation of the apparatus that the dichloroacetic acid for dissolving polyketone and the dichloroacetic acid in the mobile phase are the same.
なお,GPCの移動相としてテトラヒドロフラン／ジクロロ
酢酸または，クロロホルム／ジクロロ酢酸の混合溶液も
用いることができる。前記において，ポリケトンはジク
ロロ酢酸に0.2重量％程度加熱溶解後，メンブランフィ
ルタ（孔径:0.45μｍ）でろ過し，そのろ液200μＬがHP
LCに注入される。As the mobile phase of GPC, a mixed solution of tetrahydrofuran / dichloroacetic acid or chloroform / dichloroacetic acid can also be used. In the above, the polyketone was dissolved in dichloroacetic acid by about 0.2% by weight and then filtered through a membrane filter (pore size: 0.45 μm).
Injected into LC.
一方,GPCで用いる分離カラムとしては，汎用の高分子ゲ
ルを充てんしたものが使用可能であり，例えば上記のス
チレン−ジビニルベンゼン共重合体の充てんカラムが好
適な例として挙げられる。On the other hand, as a separation column used in GPC, a general-purpose polymer gel-filled column can be used. For example, the above-mentioned styrene-divinylbenzene copolymer-filled column is a suitable example.
以下，図面および測定例により本発明方法を詳細に説明
する。なお，本発明は下記の実施例に限定されるもので
はない，第１図は，この発明の方法を実施する装置の一
例の構成説明図である。この図において,1は移動相貯留
槽,2は送液ポンプ,3はマニュアルインジェクタ,4はカラ
ム,5はカラムオーブン,6は示差屈折計,7はデータ処理装
置である。Hereinafter, the method of the present invention will be described in detail with reference to the drawings and measurement examples. The present invention is not limited to the following embodiments, and FIG. 1 is a structural explanatory view of an example of an apparatus for carrying out the method of the present invention. In this figure, 1 is a mobile phase storage tank, 2 is a liquid feed pump, 3 is a manual injector, 4 is a column, 5 is a column oven, 6 is a differential refractometer, and 7 is a data processor.
移動相１からポンプ２によりあらかじめ溶離液を流し，
定常状態を作る。注入された試料は溶離液によりカラム
オーブン５中のカラム４に送られ，検出器６（示差屈折
計）により分子量分布が検出される。このデータをデー
タ処理装置７で処理し，分子量分布の計算を行う。The eluent is made to flow from the mobile phase 1 by the pump 2 in advance,
Create a steady state. The injected sample is sent to the column 4 in the column oven 5 by the eluent, and the detector 6 (differential refractometer) detects the molecular weight distribution. This data is processed by the data processor 7 to calculate the molecular weight distribution.
以上装置を用いて，下記の分析条件により分析を行っ
た。Using the above equipment, analysis was performed under the following analysis conditions.
（１）分析条件 カラム;Shim−pack GPC−80 MC（（株）島津製作所製） （8mml.D.300mmL） 移動相；ジクロロ酢酸 流 量;0.5mL/min 温 度;40℃ 検出器;RID−6A（示差屈折計）（（株）島津製作所製） ポラリティ；＋ 感 度;32 10-6RIUFS 上記分析条件で分析した結果を第２図に示す。この第２
図によりGPCを用いてポリケトンが分析できることが確
認できた。(1) Analytical conditions Column: Shim-pack GPC-80 MC (Shimadzu Corporation) (8mml.D.300mmL) Mobile phase: Dichloroacetic acid Flow rate; 0.5mL / min Temperature; 40 ℃ Detector; RID -6A (differential refractometer) (manufactured by Shimadzu Corporation) Polarity; + Sensitivity; 32 10 -6 RIUFS Figure 2 shows the results of analysis under the above analysis conditions. This second
From the figure, it was confirmed that polyketone could be analyzed using GPC.
なお，第２図の縦軸は信号強度，横軸は保持時間を表
す。The vertical axis of FIG. 2 represents the signal intensity and the horizontal axis represents the holding time.
本発明は，ポリケトンの溶離液としてジクロロ酢酸を用
い,GPCの移動相としてジクロロ酢酸を用い，検出手段と
して示差屈折計を用いたGPCによって分析することによ
り，ポリケトンの分子量分布の測定を効率良く，正確に
行うことができた。The present invention uses dichloroacetic acid as an eluent of polyketone, dichloroacetic acid as a mobile phase of GPC, and analyzes by GPC using a differential refractometer as a detection means, thereby efficiently measuring the molecular weight distribution of polyketone. I was able to do it accurately.
また，この分子量分布をGPCにより，簡便に得ることが
できた。Moreover, this molecular weight distribution could be easily obtained by GPC.
さらに，得られた分子量分布によりポリケトンの品質管
理，性能評価が簡単に行えるという特別な効果を有す
る。Furthermore, the obtained molecular weight distribution has a special effect that the quality control and performance evaluation of the polyketone can be easily performed.
第１図は本発明方法を実施する装置の一例の構成説明
図，第２図は本発明ポリケトンの溶解液についての分子
量分布を表すクロマトグラムである。 1:移動相貯留相、2:送液ポンプ 3:マニュアルインジェクタ 4:カラム、5:カラムオーブン 6:示差屈折計、7:データ処理装置FIG. 1 is an explanatory view of the constitution of an example of an apparatus for carrying out the method of the present invention, and FIG. 2 is a chromatogram showing the molecular weight distribution of a solution of the polyketone of the present invention. 1: Mobile phase Stored phase, 2: Liquid transfer pump 3: Manual injector 4: Column, 5: Column oven 6: Differential refractometer, 7: Data processor
Claims (1)
この溶液をジクロロ酢酸を移動相として用いたゲルパー
ミエーションクロマトグラフィに付して分離した後，示
差屈折計で検出することを特徴とするポリケトンの分子
量分布分析法。1. A polyketone is heated and dissolved in dichloroacetic acid,
A method for analyzing the molecular weight distribution of polyketone, which comprises subjecting this solution to gel permeation chromatography using dichloroacetic acid as a mobile phase for separation, followed by detection with a differential refractometer.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP20060390A JPH076967B2 (en) | 1990-07-27 | 1990-07-27 | Molecular weight distribution analysis method for polyketone |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP20060390A JPH076967B2 (en) | 1990-07-27 | 1990-07-27 | Molecular weight distribution analysis method for polyketone |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH0484760A JPH0484760A (en) | 1992-03-18 |
| JPH076967B2 true JPH076967B2 (en) | 1995-01-30 |
Family
ID=16427111
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP20060390A Expired - Lifetime JPH076967B2 (en) | 1990-07-27 | 1990-07-27 | Molecular weight distribution analysis method for polyketone |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH076967B2 (en) |
-
1990
- 1990-07-27 JP JP20060390A patent/JPH076967B2/en not_active Expired - Lifetime
Non-Patent Citations (2)
| Title |
|---|
| Ｐｏｌｙｍｅｒ（１９８５），２６（１３），Ｐ．１９９４−２０００ |
| Ｓｐｅｃｔｒａ２０００［ＤｅｕｘＭｉｌｌｅ（１９８７），１２２，Ｐ．４０−１ |
Also Published As
| Publication number | Publication date |
|---|---|
| JPH0484760A (en) | 1992-03-18 |
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